CN103515180B - A kind of in-situ plasma glow processing method improving tungsten oxide nanometer material film field emission characteristic - Google Patents
A kind of in-situ plasma glow processing method improving tungsten oxide nanometer material film field emission characteristic Download PDFInfo
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Abstract
The present invention provides a kind of in-situ plasma glow processing method improving tungsten oxide nanometer material film field emission characteristic.The method is as the negative electrode of field emission structure using tungsten oxide nanometer material film, and is positioned in fine vacuum test chamber.First between cloudy grid or the anode and cathode of field emission structure, apply high voltage realize Field Electron Emission, then by the gas (such as Ar) of heavy atom quality and gas (the such as H of strong reducing property2) be successively incorporated between nano material film and anode, keep certain operating air pressure, recycling high voltage forms plasma glow discharge, during Flied emission, tungsten oxide nanometer material film sample is carried out in-situ treatment, is finally reached the purpose improving its field emission characteristic.The method has the advantages that use equipment is simple, place's process gases is cheap.Its threshold electric field of tungsten oxide nanometer material film after this method processes and threshold field step-down, the distributing homogeneity of Flied emission location and illuminance distribution obtain and are effectively improved.
Description
Technical field
The present invention relates to a kind of in-situ plasma glow process side improving tungsten oxide nanometer material film field emission characteristic
Method, particularly relates to have the noble gas of heavy atom quality and has the plasma in situ process side of strong reducing property gas
Method.
Background technology
Tungsten oxide nanometer material is a kind of field emission cold-cathode material having application potential.Negative electrode to be realized is applied, material
Low electric field launch and uniformity characteristics realizes being crucial.Most researcher is prepared angle from material and is solved oxidation
The low electric field of tungsten nano material and uniformity field emission characteristic problem, such as by controlling the growth of tungsten oxide nanometer material
Pattern (A.Agiral and J.G.E.Gardenier, J.Phys.Chem.C112 (2008) 15183), controls its nanometer
The stand density (F.Liu et al., Nanoscale3 (2011) 1850) etc. of structure.But above-mentioned approach is solving tungsten oxide
Limitation is there is in the aspect of nano material film field transmitting uniformity.Owing to affecting tungsten oxide nanometer yard of material emission characteristics
A lot of because have, as nano material length and pattern, the electrical conductivity of nano material, the thing phase of nano material, receive
So how the amorphous oxide layer thickness etc. of rice material outer, improve the field emission characteristic of tungsten oxide nanometer material the most still
It it is so a key issue restricting its actual application.Although current researcher has developed some carbon that can be effectively improved and has received
The post-processing technology of the field emission characteristic of mitron, (X.H.Liang et al., Appl.Phys.Lett.88 (2006) 111501；
J.G.Ok et al.,Appl.Phys.Lett.90(2007)033117；C.L.Liu,et al.,Carbon47(2009)
1158.), but owing to CNT and tungsten oxide nanometer material have the biggest structure and physical difference, so these skills
Can art be applicable to tungsten oxide nanometer material film and also cannot be come to a conclusion, and therefore exploitation one improves tungsten oxide nanometer material
The post-processing technology of stock ground emission characteristics, applies significant to advancing it on cold cathode.
Summary of the invention
Present invention aim at providing a kind of post-processing approach improving tungsten oxide nanometer material film field emission characteristic: former
Position plasma glow processes.
The basic functional principle that situ plasma glow of the present invention processes is: owing to tungsten oxide nanometer material surface is deposited
Amorphous oxide layer film and nano material at different-thickness there is also different height, big in the most same sample
There is the biggest difference in conductance or the resistance of amount nano material, causes them cannot carry out electron emission under identical electric field,
So the uniformity of its Flied emission is not ideal enough.And Ar gas plasma is for the amorphous of nanostructured surface in the present invention
Oxide layer thin layer carries out reduction processing makes the height of nanostructured reach unanimity simultaneously, and H below2Plasma again will
The amorphous oxide layer on tungsten oxide surface is reduced to the mono-crystalline structures identical with internal structure, finally makes the electricity of nano material
The property led tends to identical, thus realizes Field Electron Emission under identical electric field, reaches to effectively improve thin film field and launches
The final goal of uniformity.
A kind of in-situ plasma glow processing method being effectively improved tungsten oxide nanometer material film field emission characteristic, bag
Include following steps:
(1) first in fine vacuum chamber, using tungsten oxide nanometer material film as the negative electrode of field emission structure, then exist
Apply high voltage between the moon-grid or the two poles of the earth, male-female pole, make nano material film that Field Electron Emission to occur, then keep
Its electric field intensity is constant, continuous processing sample a period of time, to burn some the biggest nano wire, makes whole sample
The height of the nano wire in product reaches unanimity substantially；
(2) Ar inert gas plasma processes: is introduced in fine vacuum chamber by the Ar gas of certain flow, makes in vacuum chamber
Maintain certain operating air pressure.Certain highfield is applied at field emission structure two ends, so that Ar gas emitter junction on the scene
Forming plasma glow discharge between negative and positive the two poles of the earth of structure, then stationary electric field intensity is constant, during Flied emission
Tungsten oxide nanometer material film carry out continuous in-situ process, utilize the feature that the quality of Ar atom or ion is big, bombardment
The oxide layer of its nanostructured surface so that it is the thickness of oxide layer is the most thinning and makes the height of nanostructured become further
In uniformly, finally close Ar gas, the again condition of high vacuum degree of recovery system；
(3)H2Reducibility gas Cement Composite Treated by Plasma: by the H of certain flow2Introduce in fine vacuum chamber, and allow fine vacuum
The operating air pressure in chamber keeps constant.Equally, apply certain highfield at field emission structure two ends, make H2On the scene of gas
Plasma glow is formed between negative and positive the two poles of the earth of emitter part, then thin to the tungsten oxide nanometer material during Flied emission
Film carries out the continuous processing under steady electric field, utilizes the strong reducing action amorphous oxide by its surface of H atom or ion
Layer is reduced to the mono-crystalline structures identical with its internal oxidation tungsten nanostructured, is then shut off H2, then by H2Detach Gao Zhen
Cavity, the again condition of high vacuum degree of recovery system；
(4) above-mentioned Ar and H2The circulation of in-situ plasma treatment repeats several times, until in home position observation
Sample obtains Flied emission and launches image uniformly.
The present invention is applicable not only to tungsten oxide nanometer material, but also is applicable to the tools such as molybdenum oxide, ferrum oxide and copper oxide
There is the oxide-based nanomaterial of multiple valence state structure.
Field emission structure of the present invention includes Flied emission two-level structure and band grid structure etc..
Anode of the present invention includes indium dioxide (ITO) electro-conductive glass, fluorescent screen or sheet metal electrode etc..
Ar inert gas plasma treatment technology of the present invention, the noble gas being passed through fine vacuum chamber not only wraps
Including Ar gas, also include stable chemical nature, other noble gas that atomic mass is bigger, such as N2, Kr, Xe and
Rn etc..
H of the present invention2Reducibility gas plasma treatment technique, is passed through the reducibility gas in fine vacuum chamber not only
Including H2Gas, also includes other strong reducing property gas that chemical property is active, such as H2S、NH3And B2H6Deng.
When in step 1 of the present invention, constant voltage processes, the vacuum in fine vacuum chamber need to be better than 2 × 10-4Pa, in constant voltage processing procedure
Electric current density must can bear the low 1/4-1/3 of maximum current density than nanostructured, and the time that constant voltage processes is 0.5-2h.
In step 1 of the present invention, constant voltage big current processing a period of time, in order to remove tungsten oxide nanometer material film sample
The nanostructured that upper height is bigger, so that the nanowire height on whole sample tends to uniform.Science and engineering at this step
Cheng Zhong, in feds structure, the distance between negative electrode and anode is 10 μm-1cm.Sample after this step processes
The threshold electric field of product and threshold field there will be reduction, and uniformity is slightly improved.
In step 2 of the present invention, after the big current processing of constant voltage, in fine vacuum chamber, it is passed through noble gas Ar gas, its stream
Amount is 20sccm-500sccm, and the air pressure controlling vacuum chamber now by the pumping speed adjusting gas flow and vacuum pump is steady
It is scheduled on 5 × 10-3-3×10-2Pa.Between anode and cathode, now add voltage to produce the plasma glow discharge of Ar gas.
The electric field specific size applied is can bear corresponding to maximum current density (1/4-1/3) less than nano material film
Electric field intensity is advisable, and the steady electric field process time is 0.5-2h.Aura process terminates, and closes Ar gas, and recovery system is true
Reciprocal of duty cycle.The purpose of this step is by having the Ar atom of relatively thick atom quality or ion for tungsten oxide nanometer structure
Surface amorphous oxide layer performs etching stripping.Owing to tungsten oxide nanometer material can form the amorphous of different-thickness in atmosphere
Oxide layer, and the difference of amorphous oxide layer thickness can cause the conductance of tungsten oxide nanometer materials different in same sample
Rate shows the biggest difference, and therefore peeling off of amorphous oxide layer is reduced owing to improving the electrical conductivity of tungsten oxide nanometer structure
Open and threshold field, simultaneously because the etching of oxide layer and stripping make the electrical conductivity of tungsten oxide nanometer structure in sample
Reach unanimity, so the uniformity that improve its Flied emission (includes distributing homogeneity and the illuminance distribution of Flied emission location
Property).
In step 3 of the present invention, after Ar gas plasma glow in-situ treatment terminates, in fine vacuum chamber, it is passed through high reduction
Property gas H2Gas, its flow is 20sccm-500sccm, now again by adjusting taking out of gas flow and vacuum pump
Speed controls the stable gas pressure of vacuum chamber 5 × 10-3-3×10-2Pa.Between anode and cathode, now add voltage to produce H2
The plasma glow discharge of gas, steady electric field processes nano material film 0.5-2h.The electric field applied is taked to be less than
Nano material film can bear the electric field intensity corresponding to maximum current density (1/4-1/3).Aura process terminates, and closes
H2Gas, recovery system vacuum.The purpose of this step is by having the H atom of high reproducibility or ion pair tungsten oxide
The amorphous oxide layer of nanostructured surface processes so that it is electronation occurs, becomes and the crystalline substance within nanostructured
The monocrystalline that body structure is consistent, thus improve the electrical conductivity of nanostructured further, and make the electrical conductance of nano wire in sample
Reach unanimity.Owing to the oxide layer of the tungsten oxide nanometer body structure surface after Ar gas Cement Composite Treated by Plasma in step 3 also may be used
Residual can be there is, and there still have part to present to be decrystallized, so this step is the heaviest for the raising of the field emission characteristic of sample
Want.After this step processes, the threshold electric field of sample and threshold field can improve further, simultaneously the Flied emission of thin film
Uniformity also can be improved further.Preferably, the H in step 32Flow be 100-500sccm, H2Deng
Air pressure when gas ions processes is 50-500Pa.The flow of the Ar in step 2 is 100-500sccm, Ar plasma
Air pressure during process is 50-500Pa.
In step 4 of the present invention, Ar and H2The cycle-index that in-situ plasma glow processes is advisable with 1-5 time, specifically follows
Ring number of processes is by the improvement degree of the field emission characteristic (unlatching and threshold field, and field transmitting uniformity) of sample
Determine.
In-situ plasma glow processing method proposed by the invention has the advantage that and is effectively improved tungsten oxide nanometer
The field emission characteristic of material film；Method cost is the lowest, and equipment is simple；Go for other and there is different valence state
Oxide-based nanomaterial.
Accompanying drawing explanation
Fig. 1 is the operation principle schematic diagram that the plasma glow in the present invention processes technique.
Fig. 2 A and Fig. 2 B is the SEM figure of the patterned oxide tungsten nanowires array of thermal evaporation growth.
The sample 1 of Fig. 3 picked-up in situ processes the Flied emission image in the different disposal stage of technique at plasma glow,
Scale in figure is 5mm.
Fig. 4 (A) sample 1 processes the Flied emission J-E characteristic curve of different phase in plasma in situ；(B) corresponding to
FN curve.
The sample 2 of Fig. 5 picked-up in situ processes the Flied emission image in the different disposal stage of technique at plasma glow,
Scale in figure is 5mm.
Fig. 6 (A) sample 2 processes the Flied emission J-E characteristic curve of different phase in plasma in situ；(B) corresponding to
FN curve.
Fig. 7 A and Fig. 7 B be without plasma glow in-situ treatment before tungsten oxide nano TEM and
HRTEM schemes, and illustration is the SAED figure of its correspondence, and region shown in its black annulus is amorphous oxide layer；
Fig. 7 C and Fig. 7 D be the tungsten oxide nano after Ar gas plasma glow in-situ treatment TEM and
HRTEM schemes, and illustration is the SAED figure of its correspondence, and in region shown in its black annulus, the thickness of amorphous oxide layer is bright
Aobvious thinning；
Fig. 7 E and Fig. 7 F is through H2The TEM of the tungsten oxide nano after gas plasma glow in-situ treatment and
HRTEM schemes, and illustration is the SAED figure of its correspondence, the degree of crystallinity of surface oxide layer in region shown in its black annulus
Significantly improve；
Fig. 7 G and Fig. 7 H is through Ar and H2The TEM of the tungsten oxide nano after gas plasma circular treatment and
HRTEM schemes, and illustration is the SAED figure of its correspondence, and in region shown in its black annulus, the crystalline texture of surface layer is
Through reaching unanimity with its nano wire internal crystal structure.
Detailed description of the invention
The present invention is a kind of in-situ plasma glow process side improving tungsten oxide nanometer material film field emission characteristic
Method, wherein: noble gas uses Ar gas, high reducibility gas uses H2；In plasma treatment procedure
The stable gas pressure of vacuum chamber is 5 × 10-3-3×10-2Pa, vacuum when big electric current constant voltage processes and the base vacuum of system
Degree should be better than 2 × 10-4Pa；Electric field intensity applied in constant voltage and plasma treatment procedure becomes because of sample, specifically
Standard is that the Flied emission electric current density of the sample under this constant electric field strength must be closeer than nanostructured can bear maximum current
Spend low 1/4-1/3；Tungsten oxide nanometer material film sample plasma processes and the time of big electric current constant voltage process is
0.5-2h；Ar gas and H2The cycle-index that plasma glow processes is 1-5 time.
Embodiment
Below in conjunction with specific embodiment according to explaining the present invention, but these embodiments limit never in any form
The scope of the present invention.
Embodiment one: the tungsten oxide nano film sample that in-situ plasma PROCESS FOR TREATMENT uniformity is poor
The tungsten oxide with poor emission uniformity using in-situ plasma PROCESS FOR TREATMENT thermal evaporation growth method to prepare is received
Rice noodle film sample 1.The gross area of substrate is 2.8 × 2.8cm2, pattern of nanowires generally circular in shape, a diameter of 300
μm.Having 18 pattern of nanowires owing to often going on substrate with each column, therefore on substrate, total number of pattern of nanowires is
324, total emission area is 0.229cm2。
First, the tungsten oxide nanometer linear array (sample 1, see Fig. 2) that will be patterned into is as two pole field emission structure
Negative electrode, puts in fine vacuum cavity.Anode is the fluorescent screen of coating fluorescent material, and the distance between anode and cathode is 400
μm, the background vacuum of system is 2.0 × 10-5Pa.It is found that the Flied emission of original sample 1 is equal from Fig. 3 A
Even property is poor.
Secondly, the constant voltage started under the fine vacuum of the 1st step processes.Constant voltage through this step processes, tungsten oxide nano
The threshold electric field of thin film, from 6.3V/ μm, changes to 7.6V/ μm, but its brightness uniformity occur raising slightly (see
In Fig. 3 B).
And then the Ar gas in-situ plasma treatment of the 2nd step is carried out.System is first passed through Ar gas to 2-5 × 10-3Pa, then
Applying electric field between negative and positive the two poles of the earth is that 7-9V/ μm is to produce Ar plasma.Constant voltage continuous processing 1 hour, then by Ar
Gas detaches vacuum chamber, and recovery system vacuum is 2.0 × 10-5Pa.As shown in Figure 3 C, through Ar gas Cement Composite Treated by Plasma
The distributing homogeneity of the Flied emission location of rear sample occurs in that significantly raising, now the distributing homogeneity of Flied emission location by
80.3% brings up to 85.8%.
Carry out the H of the 3rd step again2Plasma glow processes.System is passed through H2To 8x10-3-1x10-2Pa, negative and positive the two poles of the earth
Between be applied for the steady electric field of 7-9V/ μm to produce H2Plasma.Stationary electric field intensity is constant, H2Gas plasma
Body continuous processing sample 1 hour, then by H2Gas detaches vacuum chamber, and recovery system vacuum is 2.0 × 10 again-5Pa。
As shown in Figure 3 D, after this processes, the Flied emission location distributing homogeneity of tungsten oxide nanometer linear array carries from 85.8%
High to 87.5%, illuminance distribution has 81.2% to bring up to 82.1%.
This time circular treatment number of times is 1 time.
Finally carry out big electric current burin-in process.In fine vacuum 2.0 × 10-5Under Pa, fix its emission constant, even
Continuous process tungsten oxide nano thin film 1h.Now it will be noted from fig. 1 that the distributing homogeneity of the Flied emission location of sample 1
Have been increased to 88%, and illuminance distribution brings up to 85.8%, and its threshold electric field and threshold field are the most slightly
Increase (seeing Fig. 4).It is contemplated that due to the height reduction of nano wire after big current processing, simultaneously at plasma
After reason, the height of nano wire also can reduce further, and we are approximately considered between negative and positive the two poles of the earth in test process
Spacing is that 400 μm are constant, so threshold electric field and the threshold field of actually sample 1 after Cement Composite Treated by Plasma should be remote
The unlatching recorded in testing less than us and threshold field.Therefore, at by the in-situ plasma glow in the present invention
The field transmitting uniformity of the tungsten oxide nanometer linear array that science and engineering skill, originally emitting performance are poor is greatly improved,
And its threshold electric field and threshold field are held essentially constant or occur reducing.
Embodiment two: the tungsten oxide nano film sample that in-situ plasma PROCESS FOR TREATMENT uniformity is poor
The tungsten oxide with preferable emission uniformity using in-situ plasma PROCESS FOR TREATMENT thermal evaporation growth method to prepare is received
Rice noodle film sample 2, verifies the feasibility of this kind of in-situ plasma treatment technique further.The gross area of substrate is
2.8×2.8cm2, pattern of nanowires generally circular in shape, a diameter of 300 μm.Owing on substrate, often row and each column have
18 pattern of nanowires, therefore on substrate, total number of pattern of nanowires is 324, and total emission area is 0.229cm2。
The tungsten oxide nanometer linear array (sample 2) that will be patterned into equally, as the negative electrode of two pole feds, is put into
In fine vacuum cavity.Anode is the fluorescent screen of coating fluorescent material, and the distance between anode and cathode is 400 μm, system
Background vacuum is 2.0 × 10-5Pa.It is found that the field emission performance of sample 2 is preferable from Fig. 5 A, Flied emission location
Distributing homogeneity reached 81.4%, and illuminance distribution is 75.74%.
Constant voltage under 1st step fine vacuum processes: the electric field intensity 5-7V/ μm between fixing negative and positive the two poles of the earth is constant, continuously
Process sample 1h.Constant voltage through this step processes, and the threshold electric field of tungsten oxide nano thin film, from 4.0V/ μm, declines
To 2.4V/ μm (seeing Fig. 6), but the distributing homogeneity of its brightness uniformity and Flied emission location does not find substantially to change
Become and improve (seeing Fig. 5 B).
2nd step Ar gas in-situ plasma glow processes: system is passed through Ar gas to 2-5x10-3Pa, then negative and positive two
Applying electric field between pole is that 7-9V/ μm is to excite Ar plasma.Constant voltage continuous processing 1 hour, then by Ar gas
Detaching vacuum chamber, recovery system vacuum is to 2.0 × 10 again-5Pa.As shown in Figure 5 C, the Flied emission location of sample point
Cloth uniformity is brought up to 83.1% by 81.4%, and brightness uniformity is the most unchanged.
The H of the 3rd step2Plasma glow processes: system is passed through H2To 8x10-3-1x10-2Pa, between negative and positive the two poles of the earth
It is applied for the steady electric field of 7-9V/ μm to produce H2Plasma.Keep electric field intensity constant, H2Gas plasma
Processing sample time is 1 hour, then by H2Gas detaches vacuum chamber, and recovery system vacuum is 2.0 × 10 again-5Pa。
As shown in Figure 5 D, in sample, the distributing homogeneity of Flied emission location improves further, and distributing homogeneity now reaches
86.5%, threshold electric field falls below 2.3V/ μm, and the field emission performance of sample persistently improves.
This time circular treatment number of times is taked to be 1 time.
Finally carry out big electric current burin-in process.In fine vacuum 2.0 × 10-5Under Pa, still apply voltage at anode and cathode two ends,
Tungsten oxide nano thin film is made to carry out Field Electron Emission.Then sample is allowed to keep its Flied emission electric current density to be less than
Big emission 1/3, keeps this electric field intensity constant, continuous processing sample 2 thin film 1h.At the aging place of big electric current
During reason, the biggest nano wire is burned out owing to bearing bigger emission current.Aging through super-high-current
After process, Ar and H2The difference of the nanowire height that plasma is brought gradually is weakened, and their height is again
Recover consistent.Now from the figure, it can be seen that the distributing homogeneity of the Flied emission location of sample 2 has been increased to 96.8%,
Almost all of Flied emission location has been involved in emission process.The illuminance distribution of nano wire film is the most unchanged simultaneously,
And its threshold electric field contrast has had descended to 3V/ μm (seeing Fig. 6) before processing.It is contemplated that in test process
The excessive distance that have estimated between negative and positive the two poles of the earth, so the actually threshold electric field of sample 2 after Cement Composite Treated by Plasma and threshold
Value electric field is more much lower than the threshold electric field of untreated front sample 2 and threshold field.The threshold electric field that after process, sample 2 is relatively low
It is permissible that performance and the performance of excellent field transmitting uniformity fully show that the in-situ plasma glow in the present invention processes technique
It is effectively improved the field emission characteristic of tungsten oxide nano thin film.Further, by the present embodiment, the present invention is also sufficed to show that
In in-situ plasma glow processing method the suitableeest for script field emission performance preferably tungsten oxide nano sample
With.
Claims (5)
1. improve an in-situ plasma glow processing method for oxide-based nanomaterial thin film field emission characteristics, including
Following steps:
(1) first in fine vacuum chamber, using oxide-based nanomaterial thin film as the negative electrode of field emission structure, coat glimmering
The fluorescent screen of light powder, as anode, then applies high voltage between the moon-grid or the two poles of the earth, male-female pole, makes nano material thin
There is Field Electron Emission in film, then keeps its electric field intensity constant, and continuous processing sample a period of time, to burn certain
The biggest a little nano wires, make the height of the nano wire in whole sample substantially reach unanimity；
(2) inert gas plasma processes: the noble gas that flow is 20sccm-500sccm is introduced fine vacuum chamber
In, make vacuum chamber maintains 5 × 10-3-3×10-2The operating air pressure of Pa, applies certain forceful electric power at field emission structure two ends
, so that noble gas forms plasma glow discharge between negative and positive the two poles of the earth of field emission structure, the most constant
Electric field intensity is constant, the oxide-based nanomaterial thin film during Flied emission is carried out continuous in-situ process, utilizes inertia
The feature that the quality of gas atom or ion is big, bombards the oxide layer of its nano-material surface so that it is the thickness of oxide layer
The most thinning and make the height of nano material tend to uniform further, finally close noble gas, again recovery system
Condition of high vacuum degree, described noble gas includes Ar gas, also includes stable chemical nature, the N that atomic mass is bigger2、Kr、
Xe or Rn noble gas, constant electric field strength is nano material film Flied emission current density ratio nano material film institute
Electric field intensity corresponding during maximum current density low 1/4～1/3 that can bear, each constant voltage process the time be
0.5-2h；
(3) the reducibility gas Cement Composite Treated by Plasma that chemical property is active: the reducibility gas of certain flow is introduced height
In vacuum chamber, fine vacuum chamber is allowed to keep 5 × 10-3-3×10-2The operating air pressure of Pa, applies certain at field emission structure two ends
Highfield, make reducibility gas form plasma glow between negative and positive the two poles of the earth of feds, then to field
Oxide-based nanomaterial thin film in emission process carries out the continuous processing under steady electric field, utilizes the former of reducibility gas
The amorphous oxide layer on its surface is reduced to identical with its subscale nanostructured by the strong reducing action of son or ion
Mono-crystalline structures, is then shut off reducibility gas, then reducibility gas detaches fine vacuum chamber, the height of recovery system again
Vacuum, described reducibility gas not only includes H2Gas, also includes the H that chemical property is active2S、NH3Or B2H6
As reducibility gas, constant electric field strength is nano material film Flied emission current density ratio nano material film institute energy
Electric field intensity corresponding during maximum current density low 1/4～1/3 born, the flow of reducibility gas is
20sccm-500sccm, each constant voltage process time is 0.5-2h；
(4) above-mentioned noble gas and reducibility gas in-situ plasma treatment 1 time or circulation repeat several times,
Until the sample in home position observation obtains Flied emission launches image uniformly.
Method the most according to claim 1, it is characterised in that: described oxide-based nanomaterial includes that tungsten oxide is received
Rice material, or molybdenum oxide, or ferrum oxide, or copper oxide have the oxide-based nanomaterial of multiple valence state structure.
Method the most according to claim 1, it is characterised in that: described field emission structure includes that Flied emission two pole is tied
Structure and band grid structure.
Method the most according to claim 1, it is characterised in that: complete Gao Zhen after in-situ plasma treatment every time
Vacuum in cavity need to be better than 2 × 10-4Pa。
Method the most according to claim 1, it is characterised in that: the circulation of step 4 situ Cement Composite Treated by Plasma
Number of times is 1-5 time.
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